Preparation of spherical spinel LiMn2O4 cathode material for lithium ion batteries

A novel process is proposed for synthesis of spinel LiMn₂O₄ with spherical particles from the inexpensive materials MnSO₄, NH₄HCO₃, and NH₃H₂O. The successful preparation started with carefully controlled crystallization of MnCO₃, leading to particles of spherical shape and high tap density. Thermal decomposition of MnCO₃ was investigated by both DTA and TG analysis and XRD analysis of products. A precursor of product, spherical Mn₂O₃, was then obtained by heating MnCO₃. A mixture of Mn₂O₃ and Li₂CO₃ was then sintered to produce LiMn₂O₄ with retention of spherical particle shape. It was found that if lithium was in stoichiometric excess of 5% in the calcination of spinel LiMn₂O₄, the product had the largest initial specific capacity. In this way spherical particles of spinel LiMn₂O₄ were of excellent fluidity and dispersivity, and had a tap density as high as 1.9 g cm^–3 and an initial discharge capacity reaching 125 mAh g^–1. When surface-doped with cobalt in a 0.01 Co/Mn mole ratio, although the initial discharge capacity decreased to 118 mAh g^–1, the 100th cycle capacity retention reached 92.4% at 25°C. Even at 55°C the initial discharge capacity reached 113 mAh g^–1 and the 50th cycle capacity retention was in excess of 83.8%.     

二甲基甲酰胺中四种钕盐的电导

通过电导测量研究了四种钕盐：Nd(CF3SO3)3、Nd(ClO4)3、Nd(NO3)3和NdCl3在极性非质子溶剂DMF中的电导性质.利用线性拟合方法求得在25 ℃下Nd(CF3SO3)3和Nd(ClO4)3的极限摩尔电导率分别为278.8和 280.7 S•cm2•mol－1.用间接方法求得Nd(NO3)3 与NdCl3 的极限摩尔电导率分别为297.2和287.3 S•cm2 •mol－1.在25～65 ℃温度范围内，Nd(CF3SO3)3和Nd(ClO4)3的电导率随温度呈线性变化. Nd(NO3)3和NdCl3的电导行为表现出明显的离子缔合.     

柠檬酸铝/聚丙烯酰胺胶态分散凝胶反应动力学和机理的研究

采用粘度法研究了柠檬酸铝（AlCit)与部分水解取丙烯酰胺（HPAM）胶态分散凝胶体系的反应动力学。结果表明，胶态分散凝胶体系的交联反应是一级反应。并推导出胶态分散凝胶体系的反应动力学方程。     

羟基铝溶液及铝交联蒙脱土的研究

本文用(27)~Al NMR法和8-羟基喹啉萃取法分别研究了羟基铝溶液中十三聚铝含量的变化规律,还用X-射线衍射法研究了铝交联蒙脱土d_(001)的变化。研究结果表明,铝离子的聚合情况主要由羟铝比决定,而浓度影响不大。随着羟铝比的增加,溶液中单核铝离子含量减少,十三聚铝离子相对含量增加,所得铝交联蒙脱土的d_(001)也随之增大。参照这些变化规律、控制羟基铝溶液的组成,可以制备各种层柱状铝交联蒙脱土复合物。     

Crystallization of binary carboxylic acids characterized with streaming potential measurement

The streaming potential of supersaturated solution of binary carboxylic acids, which have even carbon atoms, was determined to characterize crystallization under different temperatures. The value of the streaming potential was related to the type and solubility of the acids and the starting temperature of crystallization, and was easily influenced by the pressure difference of the liquid or the rate of temperature decline. When the temperature was declined to the point where a crystal nucleus appeared, the streaming potential reached the minimum. Thereafter, as the temperature was sequentially lowered, some minicrystals grew, and the streaming potential presented an ascendant tendency. The higher the starting temperature of the acids saturated solution, the higher is the temperature corresponding to the streaming potential minimum. The less the carbon atoms in the acids and the greater the solubility of the acids are, the higher is the temperature of the streaming potential minimum. Copyright © 2007 John Wiley & Sons, Ltd.     

Rapid 3-dimensional shape determination of globular proteins by mobility capillary electrophoresis and native mass spectrometry

Established high-throughput proteomics methods provide limited information on the stereostructures of proteins. Traditional technologies for protein structure determination typically require laborious steps and cannot be performed in a high-throughput fashion. Here, we report a new medium throughput method by combining mobility capillary electrophoresis (MCE) and native mass spectrometry (MS) for the 3-dimensional (3D) shape determination of globular proteins in the liquid phase, which provides both the geometric structure and molecular mass information of proteins. A theory was established to correlate the ion hydrodynamic radius and charge state distribution in the native mass spectrum with protein geometrical parameters, through which a low-resolution structure (shape) of the protein could be determined. Our test data of 11 different globular proteins showed that this approach allows us to determine the shapes of individual proteins, protein complexes and proteins in a mixture, and to monitor protein conformational changes. Besides providing complementary protein structure information and having mixture analysis capability, this MCE and native MS based method is fast in speed and low in sample consumption, making it potentially applicable in top–down proteomics and structural biology for intact globular protein or protein complex analysis.

Using native mass spectrometry and mobility capillary electrophoresis, the ellipsoid dimensions of globular proteins or protein complexes could be measured efficiently.     

Atomic absorption determination of traces of cadmium in urine after electrodeposition onto a tungsten wire

A three-coil tungsten wire is used as electrode for the preconcentration of cadmium, which is then placed in a graphite tube for atomization and atomic absorption measurement. The heating parameters of the graphite furnace are optimized using the Modified and Weighted Centroid Simplex Method (MWCS), and computer program for automatic calculation. Sulphuric acid is selected as the supporting electrolyte for electrodeposition. The linear range of the calibration graph is 0.00-0.55 ng/ml. The detection limit is 0.01 ng/ml. For 0.1 ng/ml cadmium the coefficient of variation is 3.35% for ten parallel determinations. No interference occurs in the presence of more than 20 coexisting ions. Traces of cadmium in urine of normal people and in river water and the recoveries for cadmium are determined. The results are satisfactory.     

A convenient synthesis of 2-aryl substituted benzo[f] [1,2,4]triazolo[1,5-a]azepine derivatives

A convenient synthetic pathway to 2-aryl-5,6-dihydro-4H-benzo[f][1,2,4]triazolo[1,5-α]azepine derivatives 7 was developed. The synthesis was based on the cycloaddition of the 1,2,3,4-tetrahydronaphthalene a-acetoxy azo compounds 3 with Ar-CN in the presence of AlCl3 and the consecutive ring enlargement.     

人血清白蛋白荧光猝灭法测定苏丹红Ⅰ

研究了在0.1 mol·L-1 Tris-HCl缓冲溶液(pH 8.2)中,人血清白蛋白(HSA)的荧光性质以及由于苏丹红Ⅰ的存在而使HSA的荧光猝灭现象进行了研究.结果表明:当HSA溶液在280 nm波长激发时,其发射波长为337 nm.当有苏丹红Ⅰ存在时其荧光发射的强度将出现猝灭,而且荧光猝灭程度(△F)与苏丹红Ⅰ的质量浓度在0.5～7.5 mg·L-1(r=0.999 7)之间呈线性关系,方法的检出限(3Sb/k)为0.1 mg·L-1,测定限(10Sb/k)为0.5 mg·L-1,相对标准偏差(m=6,n=11)为0.7%～1.8%,加标回收率为91.9%～109.3%.     

Study of Manganese Promoter on a Precipitated Iron-Based Catalyst for Fischer-Tropsch Synthesis

The effects of Manganese(Mn)incorporation on a precipitated iron-based Fischer-Tropsch synthesis(FTS)catalyst were investigated using N_2 physical adsorption,air differential thermal analysis (DTA),H_2 temperature-programmed reduction(TPR),and M(?)ssbauer spectroscopy.The FTS perfor- mances of the catalysts were tested in a slurry phase reactor.The characterization results indicated that Mn increased the surface area of the catalyst,and improved the dispersion ofα-Fe_2O_3 and reduced its crystallite size as a result of the high dispersion effect of Mn and the Fe-Mn interaction.The Fe-Mn inter- action also suppressed the reduction ofα-Fe_2O_3 to Fe_3O_4,stabilized the FeO phase,and(or)decreased the carburization degree of the catalysts in the H_2 and syngas reduction processes.In addition,incorporated Mn decreased the initial catalyst activity,but improved the catalyst stability because Mn restrained the reoxidation of iron carbides to Fe_3O_4,and improved further carburization of the catalysts.Manganese suppressed the formation of CH_4 and increased the selectivity to light olefins(C_(2-4)~=),but it had little effect on the selectivities to heavy(C_(5 )) hydrocarbons.All these results indicated that the strong Fe-Mn interaction suppressed the chemisorptive effect of the Mn as an electronic promoter,to some extent,in the precipitated iron-manganese catalyst system.